Open gear lubricants



Jan. 20, 1959 J. F. MGGROGAN 2,870,089

OPEN GEAR LUBRICANTS Filed Oct. 29, 1956 INVENTOR. JOHN F. Mc GROGAN%Z.Z Z

ATTORNEY OPEN GEAR LUBRICANTS Application October 29, 1956, Serial No.618,949 Claims. (Cl; 252-42) This invention relates to novel lubricantsand method for their manufacture. More particularly, itis concerned withopengear lubricants which are widely used on the large, slow-moving opengears, cable drums, drag chains and other similar equipment usuallyfoundin the steel, coal, cement and construction industries.

Open gear lubricants are a distinct class of lubricants which aregenerally composed of residual petroleum stocks. The lubricants of theinstant invention are unique in that the residual asphalts are thickenedby a minimum amount of sodium soap which is formed in the lubricant in anovel way during processing. These new lubricants are superior inimportant characteristics such as. high dropping point, retention oflubricant at elevated temperatures, coverage, tackiness, and lubricityat high loads. They are suited to. the various methods of. applicationcurrently used and provide adequate lubricating for extreme pressure useunder heavily loaded. conditions, as well. as for normal service.

Itv is therefore an object of this invention to provide a novel methodof manufacturing open gear lubricating greases;

It is another object of this invention to provide. open gear lubricants.possessing high dropping point characteristics while stillmaintainingrelatively soft penetration characteristics.

It is another object of this invention. to provide open gear lubricantspossessing high temperature. retention characteristics, having highretention in static areas and flowing more freely in the gear teeth.

It is still another object of this invention to provide open gearlubricants which remain plastic and tacky at very low temperatures, andwhich may be applied by paddle or brush or which may be readily sprayedor poured at existing ambient temperatures.

It is a further object ofthis invention to provide open gear lubricantshaving extreme pressure propertieswhich provide adequate lubricationunder heavily loaded conditi-ons.

Other objects and advantages will become apparent from a reading of thespecification and the appended claims.

In accordance with the present invention, it has been discovered thatopen gear lubricants having'these desired properties may be produced byforming in situ a small amount of sodium soap in a major amount of aresidual steam refined asphalt at a temperature of from approximately190 F. to approximately 205 F., affecting a. high degree of dispersionof the soap in the asphalt during and after saponification and furtherprocessing the soapthickened asphalt at a temperature of fromapproximately 210 F. to 240 F. The desired degree of dispersion isaccomplished by mechanically mixing the components with a mixer giving ahigh degree of dispersion such as the so-called lightning" mixer, Whileat the same time continuously bubbling air through the reaction massbymeans of an air spider or similar distributing mechanism and bycontinuously removing aportion of rates atent ice 2. the mixture from.the main reaction mass, pumping it through a strainer (preferably of.about mesh size). by meansv of a. gear pump'and recycling theremovedportion ofv themixtureto-the main-reaction mass- Mixing, air blowingand. recyclingv is continued while processingatZlO. F-..t o.2.40. F.until thematerial. reaches the desiredASTM dropping point andpenetration ranges, whichmaterial will. hereinafter be termed thebasegrade lubricant. The desired ASTM dropping'points are 300*" andhigher,.while. the desired ASTM- penetration unworked. at 77 'F. rangespreferably from to- 230.

Fora betterunderstanding of the processutowhich this'invention'isdirected, reference shouldbe had to the accompanying drawing whichillustrates the process set forth above- A reaction vessel 1 is providedwith a. stirring means 2 andairline Sto-anair; distributing means 4located at the bottom ofthe reaction vessel 1. Reactant inlet lines 5,6'; and 7 for admittingasphalt, fatty acid, and. sodiumhydroxideresp'ectively are provided for the purpose of introducing'the.reactants: into the. vessel. A withdrawalline 8 at 'the'bottomof thereaction vessel 1. is provided with avalve 9 for eithercompletel'ywithdrawing the reactant mixture. through line 10 or con-' tinuously.recycling a portion of the reactant mixture through line. 11,, gear pump12, strainer 13' and recycle line 14;. backinto vessel 1.

To produce solventstliinned grade lubricants from two weight percent to40- weight percent (based on the total mixture) of. Stoddarck solvent orsimilar petroleum solvent is. added to the base grade" lubricant, but itis preferable to add about 1.0 weight percent solvent for summer: useand about 13 weight percent for winter use. The'penetration of thesolvent-thinned grades rangesfrom 320 to 400 for'tlie grades whichcontain from 10 per cent to. 1-3 percent thinning solvent. Base gradesare generally applied with paddle or brush after being moderately heatedtov about 150 F. to 200 F. The solvent-thinned gradeszmay be applied byspraying, brushing, or pouring at existing ambient temperatures.

Prior to the instant invention resort was usually had to a pre-oxidizedasphalt which was then thickened with a. relatively large. amount. ofsoap in order to obtain greases having relatively high dropping points.This necessitated airblowing' the asphalt for a prolonged period; oftime. at excessively high temperatures ranging from 450 F. to 600 R,which treatment not only required special and expensive'equipmentbutalso tended to degrade the asphalt by oxidation.

It was found that. only a minimum amount of soap is required to thickenthe asphalt to the desired dropping point by forming thesodium soap insitu in the residual asphalt and dispersing said soap by the novelmanner of this invention. From one weight percent tofive weight percentof the, sodium soap formed in. from 95 weight percent to 99 weightpercent of the asphalt. is. suitable for this purpose, although from twoweight per cent to three weight percent of the soap is preferred.Moreover, by simultaneously mixing, air blowing, and recycling thecomponents a high degree of dispersion of the formed soap in the asphaltis effected so that the desired high dropping point isattained in arelatively short period of time and the tively lowtemperatures rangingbetween approximately 190 F. to 240 F. andrequiring no special equipmentother than the ordinary equipment normally used to produce greases.

The airblowing dispersion of the soap, hastens the removal of water andit partially oxidizes the asphalt so as to produce a product which hasthe: desiredhbody characteristics. at elevated temperatures. It is to benoted, however, that the asphalt" process may be carried on at rela-'has a threefoldeffect. It promotes the is not oxidized to the point ofquality degradation. The in sun formation of the sodium soap in theasphalt and arr blowing the mixture at a relatively low temperatureresult in a more efiicient process than those used in the past in thatall of the formed soap immediately has'an effect on the thickening ofthe asphalt,'whereas by prevlous methods of pre-oxidizing the asphaltand adding soap, a portion of the soap initially added would not haveany effect on the thickening of the asphalt. Hence, by the process ofthis invention a minimum amount of soap is required to reach the desireddropping point.

The No. 2 saturant grade asphalt used in the instant invention ispreferably a residual asphalt from a steam refined Venezuelan,Bachaquero or Lagunillas crude. These crudes are low gravity, low pourpoint, high sulfur content, high residual content, asphaltic typecrndes. The Islo. 2 saturant grade has the following ASTMspecificatrons:

D70 specific gravity e 0990+. D-92 flash, F 350 Min. D-6 loss (50 grams,hrs. at 325 F.) percent 5 Max. D-139 float at 122 F 100-150 secs.

These No. 2 saturant grade asphalts were analyzed by the method .ofRostler and Sternberg in order to characterize them further. This methodof analysis is described in the following publications: Industrial andEngineering Chemistry, 1949, volume 41, No. 5, page 598; Rubber Age,1951, volume 67, No. 5, page 559; Rubber Age, 1952, volume 70, page 735.It essentially comprises successively contacting the selected oil with(1) hexane, (2) 85% H 80 (3) 95% H S0 and (4) 120% H 80 That portion ofthe oil which is insoluble in hexane (or precipitates therefrom) isdeemed to be asphaltenes; that portion of the remaining oil which reactswith 85% H 80 is deemed to be N-base resins; that portion of theremaining oil which reacts with 95 percent H 50 is deemed to be group Iresins; that portion of the remaining oil which reacts with 120 percentH 80 is deemed to be groupII resins; and that portion of the originaloil which is not reacted upon by any of the foregoing treatments isdeemed to be composed of parafiinic hydrocarbons.

A number of asphalts had the following composition ranges by the Rostlerand Sternberg method of analysis:

Weight Weight Weight Weight Weight Percent Percent Percent PercentPercent Asphait- N-Base GronpI GroupII Saturated enes Resins ResinsResins Hydrocarbons Lazunillas saturant No.2 11.0-12.2 21.121.816.7-17.2 30. 8-318 18.1-19.9 Bachaquero saturant;

A typical Lagunillas No. the following characteristics:

Rostler and Sternberg analysis in percent by weight The fatty acids usedto form the sodium soap in the instant invention include both animal andvegetable saturated fatty acids, such as palmitic acid, stearic acid,

2 saturant grade asphalt had I etc. In general, the saturated fattyacids having from 14 to 24 carbon atoms in the molecule are satisfactorywith those having from 16 to 22 carbons being preferred. Fats, as wellas fatty acids, also may be used to form the soap, but fatty acids arepreferred because of their more rapid reaction (saponification) rate.From about 0.88 weight percent to about 4.39 weight percent of the fattyacid may be used, but it is preferred to utilize about 2.0 to 3.0 weightpercent of the fatty acid. The preferred fatty acid among those used isknown commercially as Hydrogenated Hydrex, and is composed ofhydrogenated marine fatty acids. It has the following specifications:

Iodine value 10 Maximum.

Saponification number 195 Minimum. Free fatty acids,

as percent oleic 96 Minimum. Titre, C 53 Minimum. Appearance No dirt, nofree water. Odor, typical Mild.

Commercial grade sodium hydroxide may be used for the saponificationstep. It is preferred to utilize an aqueous caustic solution. Variousconcentrations of alkali solutions may be employed. A 25 weight percentNaOH solution was found to be satisfactory. From about 0.12 weightpercent to about 0.61 weight percent of sodium hydroxide (on a drybasis) may be used, but it is preferred to utilize about 0.3 weightpercent to 0.4 weight percent of sodium hydroxide.

The solvent used for preparing the solvent thinned grade lubricants ofthe instant invention should have a moderate initial boiling point andbe falrly'close-cut in order to give an even evaporation rate in use.Any petroleum distillate having these characteristics may be used. Acommercial petroleum distillate known as Stoddard solvent was found tohave the desired characteristics. It had the following analysis, whichanalysis, however, should only be considered as a typical analysis of asuitable solvent since other solvents with somewhat higher and lowerboiling ranges are equally efiective.

ASTM D-287 API gravity at F 48.5

ASTM D-56 flash point T. C. 0., F 104 ASTM D-86 distillation:

Initial boiling point F 305 10% boiling point F 315 30% boiling point F320 50% boiling point F 325 boiling point F 330 boiling point F 345 Endpoint 375 It has been discovered that extreme pressure properties can beimparted to the base grade lubricants of this invention by incorporatingtherein certain proportions of graphite and a methyl ester of lard oil.It is known in the prior art that certain substances, especially thosewhich contain as the active ingredient either sulfur, chlorine, lead, orphosphorous compounds or mixtures of. these compounds, greatly augmentthe load carrying capacity of lubricating compositions. It is theorizedthat under high pressure between metal surfaces these chemical elementsreact with the metal to produce a coating which will sustain the load orprevent the two metals from welding together, thus precluding damage tothe mechanical parts.

To test the extreme pressure properties of an industrial lubricant ofthe type disclosed in the instant invention the Four-Gram Tirnken Testwas developed by the United States Steel Company as a standard test.This test is described in the United States Steel Companys LubricationEngineers Manual. Essentially the test is conducted in a machine inwhich a test cup is rotated againsta steel test block. A four gramsample of the grease undertest is applied by spatula to the bearing surIt is preferred face of the test cup and block. The machine is rotatedby hand until the excess grease on the" cup has been removed by the testblock. Pressures between the test members are regulated by applying asuitable load to lever arms. The test is run under a 43 pound lever loadat a mandrel speed of 800 R. P. M. for a period of 30 minutes. Failureis indicated by the appearance of the lubricant film on. the test cup orby machine chatter, smoke, overheating, or sounds that indicate d'rymetal pick up. A lubricant which supports the 43 pound lever load for atleast 30 minutes without failure is considered to be satisfactory foruse under'heavily loaded conditions.

The extreme pressure additives normally used inthe prior art were noteffective when incorporated in the base grade lubricants of the instantinvention. Lead naphthenate tended to de-gel the lubricant whichresulted in a. lowering of the dropping point. The base grade lubricantsof this invention containing chlorinated compounds and also thosecontaining sulfurized oils failed to pass the Timken test. The additionto the base grade lubricants of Methyl Lard'ate', a commercial methylester of lard oil fatty acids, gave good results in the Timken testalthough the Timken cup appeared to be bare during; the test. In orderto gain better coverage, graphite was added to the Methyl Lardatecontaining composition. It was discovered that the combination of thesetwo ingredients not only improved the coverage but extended the runningtime of the Timken test to beyond 45 minutes, the latter discovery beingquite unexpected since neither of these materials normally areconsidered to be extreme pressure additives. From one weight percent tofour weight percent graphite may be added, the preferred range beingfrom two weight percent to three weight percent based 'on the. totalcomposition. The amount of Methyl Lardate may vary from 0.5- weightpercent to weight percent based'on the-total composition, one to twoweight percent being the preferred range.

The graphite employed in the instant invention as an extreme pressureadditive may be obtained commercially. to utilize a small particle sizegraphite. A naturally occurring" small particle size graphite knowncommercially as lettinos'No. 5'4'69 graphite was found to besuitableinimproving theTimken' test results. In addition it provides a darkercoating on the lubricated surface.

The other extremepressure additive used in the. instant invention inconjunction with the graphite is a methyl ester of lard oil knowncommercially as Methyl Lardate. It has the following typicalcharacteristicsz.

Titre 30 C. Flash, C. O. C 345 F. Fire, C. O. C 380 F. Pour point 45 F.Saponification value 195 Iodine value 75 It has also been found that thebase grade lubricants may be combined'with certain petroleum lubricatingoil distillates to produce lubricantsro-f high dropping points butincreased penetration characteristics. Likewise, the

base grade lubricantto which has been added the. aforementioned extremepressure additives may be combined With the lubricating oil distillatesto increase thepenetration characteristics of the grease.

The preferred lubricating oil distillates are those having SayboltUniversal viscosities of between 90 and 110 seconds at 100 F. and A. P.I. gravities at 60 F. of about 25 F. It is also preferable that thedistillates be naphthenic in character since such oils are morecompatible with the asphaltic base. One such oil which isknown in thepetroleum industry as 100 Coastal Oil has been found to be highlysatisfactory for this purpose in amounts ranging up to 1'5 to 20 percentby weight of the final composition.

. If desired, either thebase grade lubricant towhichhas been added theabove described lubricating. oil distillate or the base grade lubricantcontaining the extreme pressure additives to which has been added thelubricating oildisti'llate may also be thinned by the addition of theabove described petroleum solvents such as Stoddard solvent in amountsbetween 2 and 40 weight percent.

The open gear lubricants of the instant invention are tested fordropping point characteristics using the ASTM test procedure designatedas D-566. The penetration unworked is tested according to ASTM D-217with the following modifications:

For the base grade lubricants, the moderately heated sample (150 F.)is'transferred to a 6 ounce penetration tin and is placed into a 77 F.bath overnight before the penetration is taken.

For the solvent-thinned lubricants, the sample is' transferred to aone-pound grease can of 3% inches diameter and allowed to stay in 77 F.bath overnight before the penetration is taken. p

The four-gram Tirnken test, previously described, when applied to theextreme pressure gradelubricants is run for a. minimum period of. 30minutes under a lever arm load of 43 pounds at a mandrel. speed of 800R. P. M.

The ASTM dropping point is the most significant of the characteristicsand is used as a control test during processing since it is. really anindication of the degree of dispersion of the soap in the asphalt. Thelubricants of the instant invention have a dropping point of from 300 F.to 400 F., preferably, although slightly lower or higher dropping pointsare not objectionable.

Theunworked penetrations of the base grade lubricants range from 190 toEli-minimum. The 10 percent solventthinned grades have unwo-rkedpenetrations of 320 to 350 minimum, while the 13 percent solvcnt-thinnedgrades range f'ronr360 to 400 minimum.

The in situ formation of the sodium soap in the asphalt and the methodfor its homogeneous dispersion which form a part ofthe instant inventionresult in products possessing unique characteristics. One such.characteristic is its unique behavior under low shear rates. This isdemonstrated by comparing pressure viscosities obtained on theunmodified No. 2 saturant grade asphalt against the soap thickenedmaterial, whichv is-- the base grade open gear lubricant of thisinvention.

TABLE I Apparent Viscosity in Poises Shear Rate Tempp, F. (Reciprocal iSeconds) No. 2 Open Gear Saturant Lubricant Base The pressure viscositydata were obtained according to ASTM method 13-1092 except that theapparatus was enclosed in a thermostattcd cabinet and the viscositieswere obtained at two elevated empcratures, 120 F. and l50'F.'.. Atlowshear rates the open gear lubricant-is much more viscous than thesaturant from which it is made; while at higher shear rates,thevi'scosities approach each other. This means that when in service thesoap thickened material would have high retention in static areas, whilein the gear teeth under high shear conditions the -rnaterial would flowmore readily to provide the film of lubricant that isneeded."

. Theliigh' temperature retention properties of the open gear lubricantsof this invention are evidenced further by the vertical plate'retentiontest (adhesion test). In this test the thickness of the lubricantcoating on a steel plate either the No. 2 are made, or the commercialsolvent-thinned residual is recorded after exposure to elevatedtemperatures. The

following table gives comparative data obtained on the open gearlubricant, the No. 2 saturant grade asphalt, and a commercialsolvent-thinned residual asphalt type grease.

This data shows the products of the instant invention have better hightemperature retention characteristics than saturant grade asphalt fromwhich they asphalt type greases.

The products of the instant invention remain plastic at very lowtemperatures as evidenced by a low temperature flexing test. In thistest, a strip of heavy aluminum foil is coated with the lubricant andplaced into a cold box where the temperature is lowered in ten degreesteps. At each step the lubricant coated aluminum strip is flexed. Thetemperature at which the lubricant cracks and flakes off is its minimumuseful temperature. This value was determined to be 10 F. for the basegrade lubricants of this invention and 40 F. for the solvent-thinnedgrades.

The instant invention may be further illustrated by the followingexamples:

Example I A 5718 pound charge of No. 2 saturant grade asphalt was pumpedinto a grease kettle and heated by steam to a temperature of 150 F. to190 F. The lightning mixer and the recycle gear pump were started andthe air blower turned on. A 150 pound charge of hydrogenated marinefatty acids (Hydrogenated Hydrex) was added to the kettle and the steamwas adjusted to raise the kettle temperature to 190 F. to 195 F. A 25percent solution of NaOH containing 21 pounds NaOH on a dry basis wasadded to the kettle. Saponification was carried on for a period of twohours at a temperature of 190 F. to 195 F. The temperature was increasedto 225 F. to 230 F., while the mixing, recycling and air blowing werecontinued. Air blowing was intermittently stopped for the incrementaladdition of 152 pounds of Pettinos No. 5469 graphite. After the additionof 61 pounds of,Methyl Lardate, mixing, recycling, and air blowing werecontinued at a temperature of 230 F. until the lubricant had an ASTMdropping point of 360 F. Heating and air blowing were discontinued atthis stage. The lubricant had the following composition, in Weightpercent, at this point in its manufacture:

No. 2 saturant grade asphalt; 93.7 Hydrogenated marine fatty acids(Hydrogenated Hydrex) 2.46 Sodium hydroxide (dry basis) 0.34 Graphite,No. 5469 2.5 Methyl Lat-date (methyl ester of lard oil) 1.0

A four-gram Timken extreme pressure test was run on the lubricant forthirty minutes without evidence of failure.

Example II Weight percent No. 2 saturant grade asphalt 97.5 Hydrogenatedmarine fatty acids (Hydrogenated Hydrex) Sodium hydroxide (dry basis)The above composition produced as in Example II had an ASTM droppingpoint of 313 F. and an unworked penetration at 77 F. of 210.

Example IV Weight percent No. 2 saturant grade asphalt 87.48Hydrogenated marine fatty acids (Hydrogenated Hydrex) 2.21 .Sodiumhydroxide (dry basis) 0.31 Stoddard solvent 10.0

The above composition produced by the method of Example II, except forthe addition of solvent, had an ASTM dropping point of 331 F. and apenetration, unworked, at 77 F. of 358.

Example V Weight percent No. 2 saturant grade asphalt 81.52 Hydrogenatedmarine fatty acids (Hydrogenated Hydrex) 2.14 Sodium hydroxide (drybasis) 0.30 Graphite, No. 5469 2.17 Methyl Lardate (methyl ester of lardoil) 0.87 Stoddard solvent 13.00

Example VI A portion of grease made in accordance with the pro cedure ofExample I and containing exactly the same percentage of ingredients withthe exception that no Stoddard solvent was added, was combined with 15percent by weight, based on the final composition, of a Coastal oilcontaining 2.5 percent by weight of graphite and 1.0 percent by weightof Methyl Lardate.

The final composition, in percent by weight, was as This grease had anunworked penetration of 319 (aver.- age) at 77 F. and passed theFour-Gram Timken extreme pressure test (over 30 minutes withoutfailure).

"In general, the amountsof'the arious ingredientsof the'compositions ofthe instant invention lie within the following ranges in percent byweight:

While this invention has been described with reference to specificexamples and details of the production and properties of thecompositions of the instant invention, it is to be understood that it isnot intended to limit the invention to such specific examples anddetails, except as hereinafter recited in the appended claims.

I claim:

1. A lubricating grease consisting essentially of a major amount of apartially oxidized liquid residual asphalt and a minor amount,sufiicient to thicken said asphalt, of the reaction products formed insaid asphalt of an hydrogenated marine fatty acid and sodium hydroxide.

2. A lubricating grease consisting essentially of a partially oxidizedmixture of the following ingredients in percent by weight based on thegrease:

No. 2 saturant grade asphalt 95-99 Hydrogenated marine fatty acids0.88-4.39 Sodium hydroxide (dry basis) 0.12-0.61

3. A lubricating grease consisting essentially of a major amount of thecomposition of claim 2 and from about 2 Weight percent to about 40weight percent based on the final composition of a petroleum solvent.

4. A lubricating grease consisting essentially of from about 87 weightpercent to about 90 weight percent of the composition of claim 2 andfrom about 10 to about 13 weight percent of a petroleum solvent.

5. A lubricating grease consisting essentially of a major amount of thegrease of claim 2 and up to 20 Weight percent based on the finalcomposition of a petroleum lubricating oil distillate.

6. A lubricating grease consisting essentially of from about 60 to about98 weight percent of the composition of claim 5 and from about 40 toabout 2 weight percent of a petroleum solvent.

7. A lubrication grease having extreme pressure properties consistingessentially of a major amount of a partially oxidized liquid residualasphalt and a minor amount, sufficient to thicken said asphalt, of thereaction products formed in said asphalt of hydrogenated marine fattyacids and sodium hydroxide, together with graphite and a methyl ester oflard oil, in minor but in sufficient amounts to impart extreme pressureproperties to the thickened asphalt.

8. A lubricating grease having extreme pressure properties consistingessentially of a partially oxidized mixture of the following ingredientsin percent by weight based on the grease:

No. 2 saturant grade asphalt 95-99 Hydrogenated marine fatty acids0.88-4.39 Sodium hydroxide (dry basis) 0.12-0.61 Graphite 1-4 Methylester of lard oil 0.5-5

9. A lubricating grease consisting essentially of a major amount of thecomposition of claim 8 and from about 2 weight percent to about 40weight percent based on the total composition of a petroleum solvent.

10. A lubricating grease having extreme pressure prop erties consistingessentially of a major amount of the grease of claim 8 and up to 20weight percent, based on the final composition, of a petroleumlubricating oil distillate.

11. A lubricating grease having extreme pressure properties consistingessentially of from about to about 98 weight percent of the composition.of claimv 10 and from about 40 to about 2weight percent of apetroleumsolvent.

12. A process for the manufacture of a lubricating grease whichcomprises saponifying in a major amount of a liquid residual asphaltminor amounts, sufficient to thicken said asphalt, of an hydrogenatedmarine fatty acid with sodium hydroxide at a temperature of fromapproximately 190 F. to approximately 205 F, air blowing, mixingandrecycling the reaction mixture during saponification until a highdegree of dispersion of the soap in said asphalt is accomplished, andcontinuing said air blowing, mixing and recycling at a tempe-rature offrom approximately 210 F. to approximately 240 F. until an ASTM droppingpoint of at least 300 F. and an unworked penetration at 77 F. rangingfrom about 190 F. to about 230 F. are attained.

13. A process for the manufacture of a lubricating grease whichcomprises saponifying in a major amount of a liquid residual asphaltminor amounts, sufiicient to thicken said asphalt, of an hydrogenatedmarine fatty acid with sodium hydroxide at a temperature of fromapproximately 190 F. to approximately 205 F., air blowing, mixing andrecycling the reaction mixture during saponification until a high degreeof dispersion of the soap in said asphalt is accomplished, continuingsaid air blowing, mixing and recycling at a temperature of fromapproximately 210 F. to approximately 240 F. until an ASTM droppingpoint of at least 300 F. and an unworked penetration at 7 70 F. rangingfrom about 190 F. to about 230 F. are attained, discontinuing heatingand air blowing and adding from about 2 weight percent to about 40weight percent of a petroleum solvent.

14. A process for the manufacture of a lubricating grease whichcomprises saponifying in from about 95 weight percent to about 99 weightpercent of a liquid residual asphalt about 0.88 weight percent to about4.39 weight percent of an hydrogenated marine fatty acid with from about0.12 weight percent to about 0.61 weight percent of sodium hydroxide ata temperature of from approximately 190 F. to approximately 205 F., airblowing, mixing and recycling the reaction mixture during saponificationuntil a high degree of dispersion of the soap in said asphalt isaccomplished, continuing said air blowing, mixing and recycling at atemperature of from approximately 210 F. to approximately 240 F. untilan ASTM dropping point of at least 300 F. and an unworked penetration at77 F. ranging from about 190 F. to about 230 F. are attained.

15. A process for themanufacture of a lubricating grease having extremepressure properties which comprises saponifying in from about 95 weightpercent to about 99 weight percent of a liquid residual asphalt about0.88 weight percent to about 4.39 weight percent of an hydrogenatedmarine fatty acid with from about 0.12 weight percent to about 0.61weight percent of sodium hydroxide at a temperature of fromapproximately F. to approximately 205 F., air blowing, mixing andrecycling the reaction mixture during saponification until a high degreeof dispersion of the soap in said asphalt is accomplished, continuingsaid air blowing, mixing and recycling at a temperature of fromapproximately 210 F. to approximately 240 F., adding incrementally fromabout 1 weight percent to about 4 weight percent of graphite with airblowing stopped during said additions, adding from about 0.5 weightpercent to about 5 weight percent of a methyl ester of lard oil, andcontinuing heating, air blowing, mixing and recycling until an ASTMdropping point of at least 300 F. and an unworked penetration at 77 F.ranging from about 190 F. to about 230 F. are attained.

(References on following page) UNITED STATES PATENTS Manley Aug. 25,1925 Brunstrum er a1. Aug. 20, 1940 Roehner et a1 Nov. 26, 1940 Gothardet al June 17, 1941 Morway et al. 2,625,510 Moore Ian. 22, 1952 Jan. 13,1953 OTHER REFERENCES plication of Lubricating b. Corp. (N. Y.), 1954,

UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No 2 ,8'70,089 January 20, 1959 John F. McGrogan It is hereby certified that errorappears in the printed specification of the above numbered patentrequiring correction and that the said Letters Patent should read ascorrected below.

Column 5, line 66, for "25 F." read 25 column 9, line 47, for

"lubrication" read u lubricating column 10, line 32, for "770 F." read m77 F. --n

Signed and sealed this 12th day of May 1959.

(SEAL) Attest:

KARL Ho AXLINE ROBERT C. WATSON Attesting Oflicer I Commissioner ofPatents

7. A LUBRICATION GREASE HAVING EXTREME PRESSURE PROPERTIES CONSISTINGESSENTIALLY OF A MAJOR AMOUNT OF A PARTIALLY OXIDIZED LIQUID RESIDUALASPHALT AND A MINOR AMOUNT, SUFFICIENT TO THICKEN SAID ASPHALT, OF THEREACTION PRODUCTS FORMED IN SAID ASPHALT OF HYDROGENATED MARINE FATTYACIDS AND SODIUM HYDROXIDE, TO GETHER WITH GRAPHITE AND A METHYL ESTEROF LARD OIL, IN MINOR BUT IN SUFFICIENT AMOUNTS TO IMPART EXTREMEPRESSURE PROPERTIES TO THE THICKENED ASPHALT.